CN1390823A - Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization - Google Patents
Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization Download PDFInfo
- Publication number
- CN1390823A CN1390823A CN 02136151 CN02136151A CN1390823A CN 1390823 A CN1390823 A CN 1390823A CN 02136151 CN02136151 CN 02136151 CN 02136151 A CN02136151 A CN 02136151A CN 1390823 A CN1390823 A CN 1390823A
- Authority
- CN
- China
- Prior art keywords
- reactor
- baffle plate
- stirring rake
- lower floor
- groove crack
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
A process and equipment for preparing arylcarboxylic acid by aralkyl oxidization is disclosed. Said equipment is composed of a combined stirrer axially installed in a pressure container, an oxidizing gas inlet unit between the middle layer and lower layer of stirring blades, and multiple baffles vertically arranged on the inner surface of reactor but with gap between baffle and inner surface. Its advantages are high dispersibility of materials, high gas processing power, high productivity, and low consumption of material and energy.
Description
Technical field
The present invention relates to a kind of method of preparing arylcarboxylic acid by aralkyl oxidization, and the oxidation reactor that is adopted, specifically, relate to dimethylbenzene under cobalt, manganese, bromine catalyst effect, in acetate solvate, pass through the gas-liquid phase reaction with air or good fortune oxygen, p xylene oxidation is become method of terephthalic acid and the reactor that is adopted, particularly whipping appts in the reactor and the baffle plate that is arranged in the reactor.
Background technology
The oxidizing reaction of dimethylbenzene is a kind of complex reaction, removes the main reaction that generates terephthalic acid, and other has side reaction to generate multiple by product: as p-Hydroxybenzaldehyde, p-methylbenzoic acid and p-tolyl aldehyde etc.In addition, acetic acid can decompose, and dimethylbenzene and solvent acetic acid all can the generating unit divided combustions, generates CO, CO
2And water.Resultant of reaction is separated out with crystallization, is suspended in the system, Gu constitute gas-liquid-three-phase system.Reaction process will be emitted a large amount of heats.This reaction generally is being provided with venting port and is better carrying out in the blended stirred reactor.
Practice and theoretical investigation prove that all the admixture in the reactor will directly influence the efficient of oxidizing reaction and the quality of product, therefore, design and a kind ofly can carry out the target that well-mixed reactor has become numerous scientist and pursued to reaction mass.Chinese patent 89102155.8 has disclosed a kind of oxidation reactor that the aralkyl oxidation prepares aromatic carboxylic acid that is used for, the technology that this patent is reported is improved traditional technology, the oxidizing gas inlet is arranged on the bottom of whipping appts, width with baffle plate changes 0.02～0.04 of reactor inside diameter into by traditional 1/12 of reactor inside diameter that is about simultaneously, thereby increased the capacity of gas in the reactor and reduced energy consumption, this patent has adopted a kind of whipping appts that is provided with two-layer blade simultaneously.Because the baffle plate of this patent is too narrow, and general reactor aspect ratio is all bigger, even two layers of blade superpower also can not mix very.The bottom granule density is bigger, even assembles, deposits; Reactant can not effectively disperse rapidly, influences speed of reaction and products distribution, and by product is increased.The capacity of its gas can't satisfy the needs of reaction fully, and mixing of materials is even inadequately.As lower floor's blade is moved down, though can improve the mixing and the size distribution of bottom, enlarged the oar spacing, partial circulating between oar can appear; Move down as the upper strata blade, then the upper strata upper space particularly may cause more uneven distribution mutually near the free surface.Therefore a kind of new oxidation reactor for preparing aromatic carboxylic acid with energy-conservation aralkyl oxidation that mixes of development research is that institute of branch of industry is very expected.
Summary of the invention
One of technical issues that need to address of the present invention are the oxidation reactors that discloses a kind of preparing arylcarboxylic acid by aralkyl oxidization, can not satisfy the needs of reaction and mixing of materials defective uniformly inadequately fully with the capacity that overcomes the gas that prior art exists;
Two of the technical issues that need to address of the present invention provide a kind of method of preparing arylcarboxylic acid by aralkyl oxidization.
Technical scheme of the present invention:
The present invention is to the structure of traditional oxidation reactor, comprises that whipping appts, baffle plate and oxidizing gas entry position carried out comprehensively optimizing and revising, and this oxidation reactor comprises:
A round shape vertical pressure vessel that is provided with the material inlet device;
A combination whipping appts that axially is installed in the described pressurized vessel, the present invention selects three kinds of different oar types, constitute three layers of combination oar, described combination whipping appts comprises: near the wide leaf stirring rake of upper strata aerofoil profile axial flow that is positioned at the reactor medium position, this oar power is lower and circulation ability is strong, has the better gas dispersive ability, to reach the purpose of homogeneous material; A near middle level remodeling turbine impeller that is positioned at the reactor lower part position, this stirring rake has stronger shearing force, and ventilation back power does not descend substantially, to the processing power of gas be ordinary straight leaf turbine 2-4 doubly, gas dispersion when helping big air flow is so that gas effectively disperses; Near lower floor's stirring rake that is positioned at the reactor bottom position, this lower floor's stirring rake employing good cycle, the aerofoil profile axial flow narrow leaf stirring rake that power is low are to guarantee that particle suspended the end of from.Special performance is separately given full play in the combination of three kinds of dissimilar blades, makes gas dispersion in the reactor, liquid mixing, and solid suspension, the mixing-dispersing property of three-phase system significantly improves.Reaction mass disperses quickly and effectively, even particle distribution, and gas processing capability increases, and gas holdup rises.Because local inhomogeneous district disappears, the entire reaction space is used more effectively, and improves the production intensity of reactor;
One for preventing to stop up, guarantee safety operation, the present invention takes the multitube sparger of annular distribution between middle level stirring rake and lower floor's stirring rake, near the oxidizing gas inlet device of lower floor's stirring rake, and air-flow is discharged downwards, and the pipe number is the 4-8 root;
A plurality ofly be vertically installed in reactor wall and leave the baffle plate gap, that be provided with the groove crack with reactor wall, the width of this baffle plate is 0.06～0.1 of a reactor inside diameter, the present invention reduces the width appropriateness of baffle plate, on baffle plate, slot simultaneously, make total width enough big, and span width is enough little, has both reduced systemic resistance, save energy consumption, avoid central whirlpool simultaneously.In two-phase and multiphase system, make the gas holdup increase reach 15-25%, over-all properties is better than stenotic baffle.
Since across-the-board regulation of the present invention the structure of reactor, comprise stirring rake, baffle plate and ventilating mode, the mixing-dispersing property of three-phase system significantly improves.Reaction mass disperses quickly and effectively, even particle distribution, and gas processing capability increases, and gas holdup rises.Because local inhomogeneous district disappears, the entire reaction space is used more effectively, and improves the production intensity of reactor, has reduced material consumption and energy consumption.
Description of drawings
Fig. 1 is the overall structure synoptic diagram of reactor of the present invention.
Fig. 2 is the stereographic map of upper strata stirring rake.
Fig. 3 is the top perspective view of middle level stirring rake.Fig. 4 is the front perspective view of middle level oar.
Fig. 5 is the top perspective view of lower floor's oar.
Fig. 6 is eight pipe ring formula gas distributor structural representations.
Fig. 7 is four pipe ring formula gas distributor structural representations.
Fig. 8 is single seam baffle plate synoptic diagram.
Fig. 9 double slit baffle plate synoptic diagram.
Figure 10 is the synoptic diagram of baffle plate end finger-type.
Figure 11 is the synoptic diagram of this production process.
Embodiment
See Fig. 1, oxidation reactor of the present invention comprises:
A round shape vertical pressure vessel 1 that is provided with material inlet device 2;
A whipping appts 3 that axially is installed in the described pressurized vessel 1, described whipping appts 3 comprises: near 301, one of a upper strata stirring rake that are positioned at reactor 1 medium position is positioned near reactor 1 lower position middle level stirring rake 302 and one and is positioned near reactor 1 bottom position lower floor's stirring rake 303.Upper strata stirring rake 301 adopts the aerofoil profile axial flow square blade that is provided with 6 high expanded area ratio blades 311, blade has specific section, central authorities are wheel hub, blade 311 is connected by floor with wheel hub, by wheel hub blade 311 is installed in the rotating shaft, as shown in Figure 2, concrete structure is disclosed by Chinese patent 92245125.7; Middle level stirring rake 302 usefulness remodeling turbine, comprise a disk 322 and 6 semicircles or the parabola shaped recessed leaf 323 that are arranged on these disk 322 outer rims, blade 323 evenly is installed on the centrifugal disc 322, and be connected with rotating shaft by disk 322, as shown in Figure 3 and Figure 4, concrete structure is disclosed by United States Patent (USP) 5791780; Lower floor's stirring rake 303 adopts the oblique oar of aerofoil profile axial flow narrow leaf, and as shown in Figure 5, this stirring rake 303 has the particular cross-section of six low expanded area ratio blades 333, and concrete structure is disclosed by Chinese patent 92245125.7.One of ordinary skill in the art can be made the whipping appts of being addressed easily according to the disclosed technology of above-mentioned patent;
One between middle level stirring rake 302 and lower floor's stirring rake 303, near the oxidizing gas inlet device 4 of lower floor stirring rake 303, preferred inlet device 4 is a kind of pipe ring formula gas distributor, comprise annular distribution pipe 401 and coupled logical distribution arms 402, as Fig. 7 or shown in Figure 8, the mouth of pipe is downward, the arm number is the 4-8 root, evenly arrange along annular distribution pipe 401, the diameter of annular distribution pipe 401 is 0.8～1.5 times of diameter of lower floor's agitating vane 303, the width between centers of the arm mouth of pipe and impeller is 0.1～0.35T, and T is reactor 1 internal diameter;
A plurality of reactor 1 inwalls that are vertically installed in, vertical uniform distribution, and leave the gap with reactor wall, be provided with the baffle plate 5 in groove crack 501, from span from 0.008～0.012T, the width of this baffle plate 5 is 0.06～0.1 times of reactor 1 internal diameter, the quantity of baffle plate 5 is 4, groove crack 501 on the baffle plate 5 can be one, also can be many, the bottom of baffle plate is provided with finger-type 502, account for 10～25% of baffle plate total height, as Fig. 8, Fig. 9 and shown in Figure 10, the effect of finger-type 502 is that more effective elimination turns round and round, and the area in groove crack 501 is 10～35% times of baffle plate, and groove crack 501 can be arranged on the middle part of baffle plate 5, the inboard or the outside.
Preparing arylcarboxylic acid by aralkyl oxidization, producing terephthalic acid as p xylene oxidation can be 190-200 ℃ in temperature of reaction in above-mentioned oxidation reactor, reaction pressure is 13-15kg/cm
2Condition under, undertaken by the oxygen-containing gas liquid-phase oxidation p-Xylol in transpirable solvent medium.Figure 11 is the synoptic diagram of this production process.Pei Zhi reaction mass in advance, wherein contain the material inlet device 2 adding reactors 1 from reactor 1 middle part such as dimethylbenzene, acetic acid, water and catalyzer, oxygen-containing gas is introduced into the inside of reactor 1 by oxidizing gas inlet device 4, and liquid oxidation thing and solvent medium are drawn by material outlet device 6.This reaction is strong thermopositive reaction, relies on the evaporation of solvent acetic acid, removes heat.The acetic acid of a large amount of evaporations by condensation in the condenser 8 that is arranged on reactor 1 top after, Returning reactor 1, non-condensable gases and water are discharged from reactive system by pipeline 9.
Adopt above-mentioned method preparing arylcarboxylic acid by aralkyl oxidization, because the choose reasonable and the configuration of paddle wheel, coupling between impeller, baffle plate, the ventpipe, coordination, mixing time is shortened, gas holdup increases, particle suspension, and what is more important, component distributes in the reactor, distributing mutually more meets the needs of oxidizing reaction.In the simulation test of the different scales that is comparable to the industrial production condition, the good result that all shows the present invention and obtained.
Claims (7)
1. preparing arylcarboxylic acid by aralkyl oxidization reactor, comprise round shape vertical pressure vessel (1), be vertically installed in reactor (1) inwall and leave the baffle plate (5) in gap, a whipping appts (3) and an oxidizing gas inlet device (4) that axially is installed in the pressurized vessel (1), it is characterized in that with reactor (1) inwall:
Said whipping appts (3) comprising:
A near upper strata stirring rake (301) that is positioned at reactor (1) medium position, one is positioned near reactor (1) lower position middle level stirring rake (302) and one and is positioned near the lower floor's stirring rake (303) of reactor (1) bottom position;
Said oxidizing gas inlet device (4) is positioned between middle level stirring rake (302) and the lower floor's stirring rake (303), close lower floor stirring rake place;
Said baffle plate (5) is provided with groove crack (501), and the width of baffle plate (5) is 0.06～0.1 times of reactor (1) internal diameter, and the bottom of baffle plate is provided with finger-type (502).
2. reactor as claimed in claim 1 is characterized in that: upper strata stirring rake (301) adopts the Chinese patent 92245125.7 disclosed aerofoil profile axial flow square blades that are provided with 6 high expanded area ratio blades (311);
Middle level stirring rake (302) adopts United States Patent (USP) 5791780 disclosed 6 semicircles or parabola shaped recessed leaf (323) the remodeling turbine oars that comprise a disk (322) and be arranged on this disk (322) outer rim;
Lower floor's stirring rake (303) adopts the Chinese patent 92245125.7 disclosed oblique oars of aerofoil profile axial flow narrow leaf that are provided with 6 low expanded area ratio blades (333).
3. reactor as claimed in claim 1, it is characterized in that: said inlet device (4) comprises annular distribution pipe (401) and coupled logical distribution arms (402), the mouth of pipe is downward, the arm number is the 4-8 root, evenly arrange along annular distribution pipe (401), the diameter of annular distribution pipe (401) is 0.8～1.5 times of diameter of lower floor's agitating vane (303), and the width between centers of the arm mouth of pipe and impeller is 0.1～0.35T.
4. reactor as claimed in claim 1, it is characterized in that: the groove crack (501) on the baffle plate (5) can be one or more, the area in groove crack (501) is 10～35% of a baffle plate, groove crack (501) is arranged on middle part, inboard or the outside of baffle plate (5), and the gap between baffle plate (5) and the reactor wall is 0.008～0.012T.
5. reactor as claimed in claim 2, it is characterized in that: the groove crack (501) on the baffle plate (5) can be one or more, the area in groove crack (501) is 10～35% of a baffle plate, groove crack (501) is arranged on middle part, inboard or the outside of baffle plate (5), and the gap between baffle plate (5) and the reactor wall is 0.008～0.012T.
6. reactor as claimed in claim 5 is characterized in that: the finger-type (502) of baffle plate (5) bottom accounts for 10～25% of baffle plate total height.
7. the method for a preparing arylcarboxylic acid by aralkyl oxidization, it is characterized in that: this method is included in the arbitrary described oxidation reactor of claim 1～6, by the reactions steps of the oxygen-containing gas liquid-phase oxidation p-Xylol in transpirable solvent medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136151 CN1243704C (en) | 2002-07-22 | 2002-07-22 | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02136151 CN1243704C (en) | 2002-07-22 | 2002-07-22 | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1390823A true CN1390823A (en) | 2003-01-15 |
| CN1243704C CN1243704C (en) | 2006-03-01 |
Family
ID=4748527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02136151 Expired - Fee Related CN1243704C (en) | 2002-07-22 | 2002-07-22 | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1243704C (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198390A (en) * | 2010-03-26 | 2011-09-28 | 中国石油天然气股份有限公司 | Inner circulating type ethene polymerization reaction vessel for slurry process |
| CN102532504A (en) * | 2011-12-16 | 2012-07-04 | 化学工业第二设计院宁波工程有限公司 | Synthetic reaction kettle suitable for preparation of carbon dioxide-epoxypropane copolymer |
| CN103038261A (en) * | 2010-07-30 | 2013-04-10 | 道达尔研究技术弗吕公司 | Use of a catalyst slurry preparation system |
| CN103146564A (en) * | 2012-12-03 | 2013-06-12 | 华东理工大学 | Coaxial different-speed combined oar reactor and industrial application thereof |
| CN103223325A (en) * | 2013-05-07 | 2013-07-31 | 南通大力化工设备有限公司 | Mechanical agitator of reaction vessel |
| CN104707510A (en) * | 2013-12-13 | 2015-06-17 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and polymer solution processing method |
| CN105711995A (en) * | 2016-03-17 | 2016-06-29 | 扬州市驰城石油机械有限公司 | Mud storage tank in landing-free treatment process of drilling mud |
| CN109200984A (en) * | 2018-10-18 | 2019-01-15 | 方期洲 | A kind of reaction kettle with double-radiation function function |
| CN109200983A (en) * | 2018-10-18 | 2019-01-15 | 方期洲 | A kind of highly effective reaction kettle for accelerating radiating rate |
| CN109806835A (en) * | 2019-01-31 | 2019-05-28 | 森松（江苏）重工有限公司 | A kind of novel PTA oxidation reactor |
| CN110385066A (en) * | 2019-07-30 | 2019-10-29 | 北矿机电科技有限责任公司 | High concentration large size ore pulp is sized mixing stirred tank |
| CN112805085A (en) * | 2018-10-15 | 2021-05-14 | 韩华思路信(株) | Batch reactor |
-
2002
- 2002-07-22 CN CN 02136151 patent/CN1243704C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102198390A (en) * | 2010-03-26 | 2011-09-28 | 中国石油天然气股份有限公司 | Inner circulating type ethene polymerization reaction vessel for slurry process |
| CN103038261A (en) * | 2010-07-30 | 2013-04-10 | 道达尔研究技术弗吕公司 | Use of a catalyst slurry preparation system |
| CN103038261B (en) * | 2010-07-30 | 2015-05-06 | 道达尔研究技术弗吕公司 | Use of a catalyst slurry preparation system |
| CN102532504A (en) * | 2011-12-16 | 2012-07-04 | 化学工业第二设计院宁波工程有限公司 | Synthetic reaction kettle suitable for preparation of carbon dioxide-epoxypropane copolymer |
| CN103146564A (en) * | 2012-12-03 | 2013-06-12 | 华东理工大学 | Coaxial different-speed combined oar reactor and industrial application thereof |
| CN103223325A (en) * | 2013-05-07 | 2013-07-31 | 南通大力化工设备有限公司 | Mechanical agitator of reaction vessel |
| CN104707510B (en) * | 2013-12-13 | 2017-01-18 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and polymer solution processing method |
| CN104707510A (en) * | 2013-12-13 | 2015-06-17 | 中国石油化工股份有限公司 | Liquid-liquid mixing device and polymer solution processing method |
| CN105711995A (en) * | 2016-03-17 | 2016-06-29 | 扬州市驰城石油机械有限公司 | Mud storage tank in landing-free treatment process of drilling mud |
| CN112805085A (en) * | 2018-10-15 | 2021-05-14 | 韩华思路信(株) | Batch reactor |
| CN109200984A (en) * | 2018-10-18 | 2019-01-15 | 方期洲 | A kind of reaction kettle with double-radiation function function |
| CN109200983A (en) * | 2018-10-18 | 2019-01-15 | 方期洲 | A kind of highly effective reaction kettle for accelerating radiating rate |
| CN109200983B (en) * | 2018-10-18 | 2021-05-14 | 滨州海川生物科技股份有限公司 | Efficient reaction kettle capable of accelerating heat dissipation speed |
| CN109200984B (en) * | 2018-10-18 | 2021-05-18 | 安达辉煌生物医药科技有限公司 | Reation kettle with dual heat dissipation function |
| CN109806835A (en) * | 2019-01-31 | 2019-05-28 | 森松（江苏）重工有限公司 | A kind of novel PTA oxidation reactor |
| CN109806835B (en) * | 2019-01-31 | 2024-01-05 | 森松（江苏）重工有限公司 | Novel PTA oxidation reactor |
| CN110385066A (en) * | 2019-07-30 | 2019-10-29 | 北矿机电科技有限责任公司 | High concentration large size ore pulp is sized mixing stirred tank |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1243704C (en) | 2006-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1243704C (en) | Process and oxidizing reactor for preparing arylcarboxylic acid by aralkyl oxidization | |
| CN100376321C (en) | Apparatus for and method of producing aromatic carboxylic acids | |
| CN100582079C (en) | Oxidation reactor for producing polybasic carboxylic acid | |
| JP5437805B2 (en) | Gas-liquid reactor equipment | |
| CN102358760B (en) | Stirred tank reactor | |
| US7887765B2 (en) | Reactor for the efficient oxidation of alkyl aromatic compounds | |
| CN100999458B (en) | Oxidation reactor for producing terephthalic acid | |
| TW539667B (en) | Improved agitation system for alkylbenzene oxidation reactors | |
| JP2507839B2 (en) | Stirrer | |
| US5211924A (en) | Method and apparatus for increasing conversion efficiency and reducing power costs for oxidation of an aromatic alkyl to an aromatic carboxylic acid | |
| CN100584445C (en) | Stirring/flow-guiding multi-phase reactor | |
| CN201482481U (en) | Self-suction exhaust type stirring reactor | |
| CN211586169U (en) | Heating agitator tank | |
| CN2839283Y (en) | Large polyfurnace for chloroethene mass polymerization | |
| CN2707362Y (en) | Disc reactor | |
| CN201136843Y (en) | High-efficiency gas-liquid reactor for producing acetic anhydride form liquid-phase carbonyl of methyl acetate | |
| CN204073996U (en) | A kind of wide ribbon sawtooth agitator | |
| CN205850826U (en) | A kind of outer circulation type alkylation reactor strengthening conveying | |
| CN112246209A (en) | Stirrer for reaction kettle under condition of no baffle | |
| CN105921091B (en) | One kind esterification degumming sulfonation reactor | |
| CN212882423U (en) | Closed organic chemical reaction kettle | |
| CN205627930U (en) | Extrinsic cycle formula alkylation reaction ware | |
| CN2920389Y (en) | Polyisobutylene polymerization kettle | |
| CN213590210U (en) | Mixed flow bidirectional stirrer | |
| CN218250283U (en) | Reaction kettle device capable of improving reaction rate of raw materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20060301 Termination date: 20100722 |